CN104111288A - Method for measuring siloxane small molecules in composite insulator silicone rubber - Google Patents
Method for measuring siloxane small molecules in composite insulator silicone rubber Download PDFInfo
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Abstract
A method for measuring siloxane small molecules in composite insulator silicone rubber comprises the following steps: (1) preparing a silicone rubber sample, washing off the contamination on the surface of the silicone rubber sample with absolute ethanol, drying the silicone rubber sample in a vacuum drying cabinet until the weight does not change any more; using n-hexane to extract the sample, condensing the extract, introducing the condensed solution into a gas chromatography-mass spectrum (GC-MS) instrument so as to obtain a color chromatography (GC) map; (2) analyzing each peak in the GC map to obtain corresponding mass spectrum (MS) maps, comparing the maps with the NIST08 MS data, which has been stored in a computer, so as to identifying the kinds of the small molecules; (3) carrying out GC map normalization by using the software installed in the GC-MS instrument to obtain the relative peak areas of each peak so as to obtain the relative contents of each kind of small molecular. The method can effectively identify the kinds of small molecules in composite simulator silicone rubber and measure the relative contents of the small molecules, and thus provides strong data support for evaluation on hydrophobicity recovering ability of composite insulator.
Description
Technical field
The present invention relates to a kind of micromolecular method of siloxane in mensuration composite insulator silicon rubber, especially relate to a kind of method that gas chromatography-mass spectrography is measured the little molecular species of silicon rubber siloxane and content in composite insulator.
Background technology
High-temperature silicon disulfide rubber composite insulator is insulator of new generation, has very good resistance to aging, hydrophobic nature, anti-flammability and hydrophobic restorative.Composite insulator starts large-scale application in electric system the seventies in last century; it is partly comprised of glass-epoxy leading-drawing rod, full skirt, gold utensil, adhesive linkage etc.; wherein full skirt belongs to external insulation part; can protect plug to avoid the erosion of external environment, what full skirt was used is silastic material.Therefore compare the advantage that has self uniqueness with traditional inorganic material insulator, wherein the most outstanding is exactly that hydrophobic is restorative, and this characteristic has promoted the engineering using value of composite insulator greatly.Yet in actual motion, the impact due to factors such as ultraviolet irradiation, creepage trace, acid or alkali environments, causes the aging rear forfeiture hydrophobic nature of composite insulator and hydrophobic restorative.Thereby there is insulator, fall string accident, affect the normal operation of electric system, to productive life, cause huge economic loss.
At present, the Performance Evaluation to composite insulator, rests on the pycnometric stage.The method requires very high to tester's experience, and error is larger.By literature search, the assay method that there is no so far a kind of science both at home and abroad.If can find a kind of quantitative evaluating method of composite insulator silicon rubber performance, can be significant for productive life.
Gas chromatography ceremony refers to the chromatograph as mobile phase with gas, is isolated the advantages such as sensitivity for analysis is high, applied range that it has according to the difference of the boiling point of analyte, polarity and adsorbability.But but accurate not in structure analysis.Mass spectrometer is in high vacuum system, by substance ion, then particle is sent into magnetic field, and be isolated according to the specific charge of ion with high energy particle, then measures the intensity of various ions, and finally obtains the abundant structural information of material.
Gas chromatograph-mass spectrometer (GCMS) (GC-MS) combines the advantage of the efficient separating power of gas chromatography (GC) and mass spectrometer (MS) analytical structure.Be widely used in the fields such as petrochemical complex, clinical chemistry, environmental monitoring and traditional Chinese medicine ingredients analysis.The electron impact mass spectra of gas chromatography-mass spectrum can after the abundant information of the structure of matter is provided, and accumulated for many years the mass spectrometric data of a large amount of standard substances, for automated analysis provides may.For volatile little molecule and half volatile micromolecular compound, gas chromatograph-mass spectrometer (GCMS) is the sharp weapon of analyzing.
Silicon rubber compound insulator is in the process of refining, and the content of rubber medium vinyl has determined to have in finished product some does not have the little molecule of crosslinked siloxane.In existing theory, little molecular migration has played key effect in silicon rubber hydrophobic rejuvenation.By the extracting little molecular melting of normal hexane, with gas chromatography-mass spectrography, analyze extract, can obtain little molecular species and relative content information, for the hydrophobic of assessment silicon rubber is restorative, provide strong data supporting, and the method is easy and simple to handle, relative error is little, has application value realistic.
Summary of the invention
Technical matters to be solved by this invention, is just to provide a kind of micromolecular method of siloxane in mensuration composite insulator silicon rubber, and the method is quick, accurate, easy to operate and relative error is little, has application value realistic.
Solve the problems of the technologies described above, the technical solution used in the present invention is:
The micromolecular method of siloxane in mensuration composite insulator silicon rubber, is characterized in that comprising the following steps:
It is some that S1 gets silicon rubber sample, cleans the surperficial dirt of sample with absolute ethyl alcohol, puts into vacuum drying chamber dry, dry set temperature: 65 ℃, drying time, 5h, weighed after dry end; Repeat the above step that is dried, weighs, twice of front and back number percent of poor quality, within 0.15%, thinks that sample reaches constant weight, records the quality (m that finally weighs
0);
S2 puts into Soxhlet extraction device by dried sample and soaks extraction with normal hexane, after extracting, takes out silicon rubber sample and puts into vacuum drying chamber, set temperature: 65 ℃, drying time, 24h, weighed after being dried, recording quality (m
1), the relative weight loss rate (m of calculating silicon rubber sample
1-m
0)/m
0, (specifically seeing Fig. 1), when the fluctuation range of the twice relative weight loss rate in front and back is in 0.001, thought and reached constant weight;
S3 is used Rotary Evaporators that the solution after extracting is concentrated into 3mL; (consumption of sample does not have the upper limit, does not affect measurement below; Sample is more, and the solution after concentrated is denseer, but the relative content of each solute component fix, what we measured is exactly the relative content of each little molecule solute; The 3mL here can change certain scope into, as 1-5mL, is mainly the error being caused by operation, does not affect the measurement of relative content below.)
S4 adopts Splitless injecting samples analysis by the solution after concentrated in gas chromatograph-mass spectrometer (GCMS), and single injected sampling amount is 1 μ L, obtains chromatogram (GC) collection of illustrative plates; Resolve each peak amplifying in chromatogram (GC) collection of illustrative plates and obtain corresponding mass spectrogram, mark peak position; Get a certain definite peak, according to retention time, peak figure is amplified, obtain its mass spectrogram; Through the contrast of row fingerprint, determine micromolecular kind with existing NIST08 spectrum spectrum library in computing machine;
GCMS for S5 (gas chromatograph-mass spectrometer) carries software by the normalization of chromatogram (GC) collection of illustrative plates, calculate total peak area and the peak area at each peak, with the peak area at each peak, divided by total peak area, obtain the relative peak area at each peak again, this relative peak area characterizes relative content, has obtained the corresponding micromolecular relative content in each peak.
The parameter of the gas chromatography-mass spectrum in described step S4 is as follows:
Chromatographic column: VF-5ms chromatographic column;
Temperature programme pattern: 50 ℃ of initial temperatures, keep 3min, then the speed with 2 ℃/min is warming up to 290 ℃, keeps 10min;
Injector temperature: 300 ℃;
Solvent delay: 3.5min;
Chromatography-mass spectroscopy interface temperature: 260 ℃;
Carrier gas: helium, purity >=99.999%, flow velocity: 1mL/min;
MS: ion source temperature: 200 ℃; Ionization mode: EI; Ionizing energy: 70eV; Mass scanning scope: (30-2000) m/z (amu).
Beneficial effect: the present invention can be quick, easy obtains the micromolecular kind of siloxane and relative content in composite insulator silicon rubber, for the performance of assessment silicon rubber provides foundation.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further elaborated.
Fig. 1 silicon rubber weightlessness is with extracting time variation diagram;
Fig. 2 formula silicon rubber chromatogram (GC) collection of illustrative plates;
Peak 1 mass spectrogram in Fig. 3 chromatogram (GC) collection of illustrative plates;
The little molecular species figure of Fig. 4 formula silicon rubber;
The small molecular phase of Fig. 5 formula silicon rubber is to containing spirogram;
Fig. 6 is silicon rubber chromatogram (GC) collection of illustrative plates of aluminium hydroxide not;
Fig. 7 not the silicon rubber small molecular phase of aluminium hydroxide to containing spirogram.
Embodiment
The micromolecular method of siloxane in mensuration composite insulator silicon rubber of the present invention, comprises the following steps:
S1 gets 10, silicon rubber sample, with absolute ethyl alcohol, cleans after sample surfaces dirt, is put in vacuum drying mutually dry; Dry set temperature: 65 ℃, drying time, 5h, weighed after dry end; Repeat the above-mentioned step that is dried, weighs, until twice of front and back weighting error, in 0.002g, thinks that sample reaches constant weight; Record the quality (m that finally weighs
0).
S2 puts into Soxhlet extractor by sample and carries out extracting
For the organic solvent that extracts, have a lot, as chloroform, sherwood oil etc., this experimental is except the larger chloroform of toxicity and the large potpourri sherwood oil of boiling point span, selected utmost point hypotoxicity, boiling point is lower and extraction rate was acquired is good normal hexane to soak extraction; After extracting, take out silicon rubber sample and put into vacuum drying chamber, set temperature: 65 ℃, drying time, 24h, weighed after being dried, recording quality (m
1), the relative weight loss rate (m of calculating silicon rubber sample
1-m
0)/m
0, to constant weight, as Fig. 1.
S3 is concentrated into 3mL with Rotary Evaporators by the solution after extracting;
Then S4 adopts Splitless injecting samples analysis in gas chromatograph-mass spectrometer (GCMS), and single injected sampling amount is 1 μ L, obtains chromatogram (GC) collection of illustrative plates;
The parameter that gas chromatography-mass spectrum is set is as follows:
Chromatographic column: VF-5ms chromatographic column;
Temperature programme pattern: 50 ℃ of initial temperatures, keep 3min, then the speed with 2 ℃/min is warming up to 290 ℃, keeps 10min;
Injector temperature: 300 ℃;
Solvent delay: 3.5min;
Chromatography-mass spectroscopy interface temperature: 260 ℃;
Carrier gas: helium, purity >=99.999%, flow velocity: 1mL/min;
MS: ion source temperature: 200 ℃; Ionization mode: EI; Ionizing energy: 70eV; Mass scanning scope: (30-2000) m/z (amu).
Described extracting normal hexane is to analyze pure rank.
According to chromatogram (GC) collection of illustrative plates, obtain retention time and the intensity at each peak, and mark peak position, as Fig. 2; Get a certain definite peak, according to retention time, peak figure is amplified, obtain mass spectrogram, as Fig. 3; The mass spectrogram obtaining is mated through row with existing NIST08 mass spectrum picture library in computing machine, to determine micromolecular kind, see Fig. 4;
S5 carries software by the normalization of chromatogram (GC) collection of illustrative plates with GCMS, obtain total peak area and the peak area at each peak, with the peak area at each peak, divided by total peak area, obtain the relative peak area at each peak again, this relative peak area characterizes relative content, has obtained the corresponding micromolecular relative content in each peak.Fig. 5 is micromolecular relative content figure.
Specific embodiment 1
1,10, the silicon rubber sample of aluminium hydroxide not, specification is 2cm * 2cm * 1mm.With after absolute ethyl alcohol clean surface dirt, be put in vacuum drying mutually dry.Set temperature: 65 ℃, drying time 5h.After dry end, weigh.Repeat above-mentioned steps, until twice of front and back weighting error, in 0.002g, thinks that sample reaches constant weight.Record the quality (m that finally weighs
0).
2, sample is put into Soxhlet extractor and is carried out extracting, select normal hexane to carry out, after extracting, take out silicon rubber sample and put into vacuum drying chamber, set temperature: 65 ℃, drying time 24h.After dry, weigh, recording quality (m
1).Calculate the relative weight loss rate (m of silicon rubber sample
1-m
0)/m
0, to constant weight.
3, with Rotary Evaporators, 3mL will be concentrated in extract, then sample introduction in the 450-GC320-MS type gas chromatograph-mass spectrometer (GCMS) of U.S. Brooker dalton company.Optimum condition in the present invention is set, obtains chromatogram (GC) collection of illustrative plates.According to chromatogram (GC) collection of illustrative plates, obtain retention time and the intensity at each peak, and mark peak position, as Fig. 6.Get a certain definite peak, according to retention time, peak figure is amplified, obtain mass spectrogram.The mass spectrogram obtaining is mated through row with existing NIST08 mass spectrum picture library in computing machine, to determine micromolecular kind.
4, with GCMS, carry software and obtain total peak area and the peak area at each peak, then divided by total peak area, obtain the relative peak area at each peak with the peak area at each peak.This relative peak area can characterize relative content, has obtained the corresponding micromolecular relative content in each peak.See Fig. 7.
Claims (2)
1. measure the micromolecular method of siloxane in composite insulator silicon rubber, it is characterized in that comprising the following steps:
It is some that S1 gets silicon rubber sample, cleans the surperficial dirt of sample with absolute ethyl alcohol, puts into vacuum drying chamber dry, dry set temperature: 65 ℃, drying time, 5h, weighed after dry end; Repeat the above step that is dried, weighs, twice of front and back number percent of poor quality, within 0.15%, thinks that sample reaches constant weight, records the quality (m that finally weighs
0);
S2 puts into Soxhlet extraction device by dried sample and soaks extraction with normal hexane, after extracting, takes out silicon rubber sample and puts into vacuum drying chamber, set temperature: 65 ℃, drying time, 24h, weighed after being dried, recording quality (m
1), the relative weight loss rate (m of calculating silicon rubber sample
1-m
0)/m
0, when the fluctuation range of the twice relative weight loss rate in front and back is in 0.001, think and reach constant weight;
S3 is used Rotary Evaporators that the solution after extracting is concentrated into 3mL;
S4 adopts Splitless injecting samples analysis by the solution after concentrated in gas chromatograph-mass spectrometer (GCMS), and single injected sampling amount is 1 μ L, obtains chromatogram collection of illustrative plates; Each peak of resolving in expansive color spectrogram spectrum obtains corresponding mass spectrogram, marks peak position; Get a certain definite peak, according to retention time, peak figure is amplified, obtain its mass spectrogram; Through the contrast of row fingerprint, determine micromolecular kind with existing NIST08 spectrum spectrum library in computing machine;
S5 carries software by the normalization of chromatogram collection of illustrative plates with GCMS, calculate total peak area and the peak area at each peak, with the peak area at each peak, divided by total peak area, obtain the relative peak area at each peak again, this relative peak area characterizes relative content, has obtained the corresponding micromolecular relative content in each peak.
2. the micromolecular method of siloxane in mensuration composite insulator silicon rubber according to claim 1, is characterized in that: the parameter of the gas chromatography-mass spectrum in described step S4 is as follows:
Chromatographic column: VF-5ms chromatographic column;
Temperature programme pattern: 50 ℃ of initial temperatures, keep 3min, then the speed with 2 ℃/min is warming up to 290 ℃, keeps 10min;
Injector temperature: 300 ℃;
Solvent delay: 3.5min;
Chromatography-mass spectroscopy interface temperature: 260 ℃;
Carrier gas: helium, purity >=99.999%, flow velocity: 1mL/min;
MS: ion source temperature: 200 ℃; Ionization mode: EI; Ionizing energy: 70eV; Mass scanning scope: (30-2000) m/z (amu).
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105259271A (en) * | 2015-11-13 | 2016-01-20 | 广东电网有限责任公司电力科学研究院 | Method for quantitatively testing total concentration of small molecules in composite insulator silicone rubber |
| CN105424837A (en) * | 2015-12-10 | 2016-03-23 | 北京彤程创展科技有限公司 | Analysis method of organic additives in rubber and plastic auxiliaries with rubber as carriers |
| CN105548387A (en) * | 2015-12-10 | 2016-05-04 | 北京彤程创展科技有限公司 | Identification method for phenol-formaldehyde resin in rubber and rubber chemicals |
| CN106442847A (en) * | 2016-11-10 | 2017-02-22 | 广东电网有限责任公司电力科学研究院 | Method for determining dirt ingredients on insulator surface |
| CN111610249A (en) * | 2020-06-01 | 2020-09-01 | 国网湖南省电力有限公司 | Method for evaluating aging state of high-temperature vulcanized silicone rubber |
| CN111781294A (en) * | 2020-06-04 | 2020-10-16 | 上海市质量监督检验技术研究院 | Method for detecting content of decamethylcyclopentasiloxane and dodecamethylcyclohexasiloxane in textile |
| CN115452975A (en) * | 2022-08-26 | 2022-12-09 | 浙江新安化工集团股份有限公司 | Method for measuring content of cyclosiloxane in polyether modified silicone oil |
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Cited By (9)
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| CN105259271A (en) * | 2015-11-13 | 2016-01-20 | 广东电网有限责任公司电力科学研究院 | Method for quantitatively testing total concentration of small molecules in composite insulator silicone rubber |
| CN105424837A (en) * | 2015-12-10 | 2016-03-23 | 北京彤程创展科技有限公司 | Analysis method of organic additives in rubber and plastic auxiliaries with rubber as carriers |
| CN105548387A (en) * | 2015-12-10 | 2016-05-04 | 北京彤程创展科技有限公司 | Identification method for phenol-formaldehyde resin in rubber and rubber chemicals |
| CN105548387B (en) * | 2015-12-10 | 2017-12-05 | 北京彤程创展科技有限公司 | The authentication method of phenol formaldehyde resin in rubber and rubber chemicals |
| CN105424837B (en) * | 2015-12-10 | 2017-12-05 | 北京彤程创展科技有限公司 | The analysis method of organic additive in using rubber as the rubber and plastics auxiliaries of carrier |
| CN106442847A (en) * | 2016-11-10 | 2017-02-22 | 广东电网有限责任公司电力科学研究院 | Method for determining dirt ingredients on insulator surface |
| CN111610249A (en) * | 2020-06-01 | 2020-09-01 | 国网湖南省电力有限公司 | Method for evaluating aging state of high-temperature vulcanized silicone rubber |
| CN111781294A (en) * | 2020-06-04 | 2020-10-16 | 上海市质量监督检验技术研究院 | Method for detecting content of decamethylcyclopentasiloxane and dodecamethylcyclohexasiloxane in textile |
| CN115452975A (en) * | 2022-08-26 | 2022-12-09 | 浙江新安化工集团股份有限公司 | Method for measuring content of cyclosiloxane in polyether modified silicone oil |
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Address after: 510080 Dongfeng East Road, Dongfeng, Guangdong, Guangzhou, Zhejiang Province, No. 8 Co-patentee after: Wuhan University Patentee after: ELECTRIC POWER RESEARCH INSTITUTE, GUANGDONG POWER GRID CO., LTD. Address before: 510080 Dongfeng East Road, Dongfeng, Guangdong, Guangzhou, Zhejiang Province, No. 8 Co-patentee before: Wuhan University Patentee before: Electrical Power Research Institute of Guangdong Power Grid Corporation |
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